摘要
目的:建立鸡蛋中5种氨基糖苷类药物残留的UPLC-MS/MS检测方法。方法:样品经磷酸盐缓冲液提取,调节p H后,过C_(18)固相萃取小柱净化,氮气吹干后七氟丁酸溶液复溶,进行UPLC-MS/MS分析。色谱柱:BEH C_(18)(50 mm×2.1 mm,1.7μm);流动相:20 mmol·L^(-1)七氟丁酸乙腈(A)-20 mmol·L^(-1)七氟丁酸水溶液(B),梯度洗脱(0~2 min,4%A线性变化至30%A;2~4 min,30%A线性变化至60%A;4~5 min,60%A线性变化至96%A;5~5.5 min,96%A线性变化至4%A;5.5~7.0 min,维持4%A);流速:0.3 m L·min^(-1);柱温:30℃;进样量:10μL。结果:5种氨基糖苷类药物质量浓度在200~1 000 ng·m L^(-1)范围内呈现良好的线性关系,相关系数r均大于0.995;添加500 ng·g^(-1)时回收率范围为67.9%~79.4%,批内RSD范围为1.03%~4.08%,批间RSD范围为7.77%~16.50%;方法检测限为5μg·kg^(-1),定量限为20μg·kg^(-1)。20份实际鸡蛋样品中均未检出5种氨基糖苷类药物。结论:经方法学验证,本方法可用于鸡蛋中氨基糖苷类药物的检测。
Objective： To develop a UPLC-MS/MS analysis method for the determination of 5 aminoglycosides in eggs. Methods： The samples were extracted with phosphate buffer solution. After adjusting the pH value, the solution was purified with C18 solid phase extraction column, dried by nitrogen and reconstituted with seven fluorine butyric acid solution. UPLC-MS/MS analysis was then performed. The separation was carried out on a Waters BEH C18（ 50 mm × 2.1 mm, 1.7 μm ）column with gradient elution （0-2 min, 4%A linear change to 30%A; 2-4 min, 30%A linear change to 60%A; 4-5 min, 60%A linear change to 96%A; 5-5.5 min, 96%A linear change to 4%A; 5.5-7.0 min, 4%A maintained ）using acetonitrile with 20 mmol·L^-1 seven fluorine butyric acid （ A ） -20 mmol·L^-1 seven fluorine butyric acid （ B ）. The flow rate was 0.3 mL·min^-1, the column temperature 30 ℃, and the injection volume 10 μL. Results： Excellent linear relationship was obtained from 200 ng· mL^-1 to 1 000 ng· mL^-1 for the five aminoglycosides （ correlation coefficient r≥0.995 ）, the recoveries ranged from 67.9% to 79.4% at 500 ng· g^-1, and intra-and inter-batch variation coefficients were 1.03%-4.08%, and 7.77%- 16.50%, respectively. The detection limit was 5μg·kg^-1, and the limit of quantification was 20 μg·kg^-1. The five aminoglycosides were not detected in any of the 20 samples. Conclusion： The methodology validation showed that the established method is specific, simple, accurate, and rapid, which can be used to determine aminoglycosides in eggs.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2016年第2期301-305,共5页
Chinese Journal of Pharmaceutical Analysis
基金
国家支撑计划"畜禽产品安全生产监控和检测技术研究(2014BAD13B05)"
